阻燃剂三嗪三苯基次膦酸丙酯的合成与应用研究

SYNTHESIS AND APPLICATION OF FLAME RETARDANT TRIAZINE TRIPHENYL PHOSPHINIC PROPYL ESTER

以三聚氯氰和苯基次膦酸二丙酯(PPDPE)为原料,合成了一种新型有机膦阻燃剂三嗪三苯基次膦酸丙酯——2,4,6-三(O-丙基-苯基次膦酰基)-1,3,5-三嗪。合成最佳工艺条件为:n(三聚氯氰)∶n(PPDPE)=1∶3.2,在氮气保护下,将约1/3的PPDPE于50℃滴加到三聚氯氰中,反应2h;升温至70℃,再滴加1/3的PPDPE,反应2h;最后升温至85℃滴加余下的PPDPE,反应4h,收率为95.9%。采用红外光谱、核磁共振、差热分析和极限氧指数等表征了产物的结构及性能。结果表明,产物对聚对苯二甲酸丁二醇酯阻燃效能高,且与双磷酸季戊四醇酯蜜胺盐、聚氰胺氰脲酸盐复配有很好的协同阻燃效果。

A novel organic phosphorus flame retardants,triazine triphenyl phosphinic propyl ester,which was also known as 2,4,6-three（O-propyl-phenyl phosphinic acyl）-1,3,5-triazine,was synthesized by using phenylphosphinic dipropyl ester（PPDPE）and cyanuric chloride as raw materials.The optimal conditions were selected as follows：n（cyanuric chloride）∶n（PPDPE）=1∶3.2,about 1/3of PPDPE was added at 50℃ under the N2 atmosphere to react for 2h,then another 1/3of PPDPE was added at 70 ℃to react for 2h,finally the rest PPDPE was added at 85℃to react for 4h,therefore,the percentage of reaction yield can reach 95.9%.The structure and properties of the product was characterized by FT-IR,1 H NMR,TG-DTA and LOI technique.Results showed that the product had a high flame-retarded efficiency with PBT and had a good synergistic flame-retarded efficiency when remixed with MCA and MPP.